CN108424136B - MHz级开关电源用MnZn功率铁氧体及其制备方法 - Google Patents

MHz级开关电源用MnZn功率铁氧体及其制备方法 Download PDF

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CN108424136B
CN108424136B CN201810233493.1A CN201810233493A CN108424136B CN 108424136 B CN108424136 B CN 108424136B CN 201810233493 A CN201810233493 A CN 201810233493A CN 108424136 B CN108424136 B CN 108424136B
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余忠
胡鑫
孙科
郭荣迪
蒋晓娜
兰中文
吴国华
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Sunshine Electronic Technology Co ltd
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Abstract

MHz级开关电源用MnZn功率铁氧体及其制备方法，涉及电子材料技术。本发明的铁氧体由主料和掺杂剂组成，主料按照摩尔百分比计，以氧化物计算，包括：52～56mol％Fe2O3，5～11mol％ZnO，33～43mol％MnO；掺杂剂按照重量百分比，以氧化物计算，包括：0.05～0.1wt％CaCO3，0.1～0.3wt％TiO2，0.1～0.3wt％Co2O3，0.01～0.1wt％SnO2，0.01～0.1wt％V2O5。本发明有效降低了材料在MHz高频时的损耗，在0.5～3MHz的宽频范围和25～100℃的温度范围内都具有较低的功率损耗。同时，本发明提供的制备方法烧结温度低，具有节能和环保的优点。

Description

MHz级开关电源用MnZn功率铁氧体及其制备方法
技术领域
本发明涉及电子材料技术，特别涉及MnZn功率铁氧体材料。
背景技术
软磁铁氧体是一种重要的电子器件基础材料，使用软磁材料制作的磁心主要用于制造电子变压器、电感器和滤波器等。其中，MnZn功率铁氧体材料由于具有高饱和磁感应强度(Bs)、高起始磁导率(μi)及低损耗(PL)等优点，被广泛应用于开关电源变压器中。当前开关电源正向高频化、小型高效化方向发展，而随着开关电源的应用频率的逐渐增加，变压器、电感器等的损耗在不断增加，特别是在频率达到MHz后，损耗更是急剧增加，发热增大，这一定程度上阻碍了开关电源的高频化和集成化发展。因而迫切需要研制出在高频下，具有较低损耗的MnZn功率铁氧体材料。此外，节能和环保是当今世界发展要的重要主题，现有的制备MnZn功率铁氧体的技术，烧结温度为1200～1400℃，能耗较大，不利于节能和环保。
近年来，国内外各大公司相继研发出了应用于MHz高频的MnZn功率铁氧体材料，在国外，欧洲的Ferroxcube公司推出的3F4材料的起始磁导率μi＝900±20％，饱和磁感应强度Bs＝410mT(25℃)，在500kHz50mT条件下损耗为220mW/cm3(25℃)和170mW/cm3(100℃)，1MHz30mT条件下损耗为140mW/cm3(25℃)和130mW/cm3(100℃)，3MHz10mT条件下损耗为190mW/cm3(25℃)和220mW/cm3(100℃)，居里温度Tc＝220℃，电阻率ρ＝10Ω˙m，该材料的μi、Bs和居里温度都较低，损耗较高；国内目前只有少数企业能够生产应用于MHz高频的MnZn功率铁氧体，横店东磁集团推出的DMR50材料的μi＝1400±20％，Bs＝470mT(25℃)，在500kHz50mT条件下损耗为130mW/cm3(25℃)和80mW/cm3(100℃)，1MHz30mT条件下损耗为140mW/cm3(25℃)和185mW/cm3(100℃)，3MHz10mT条件下损耗为275mW/cm3(25℃)和305mW/cm3(100℃)，居里温度Tc＝240℃；天通公司(TDG)研制的TP5E材料，μi＝1200±25％，Bs＝520mT(25℃)，1MHz30mT条件下损耗为120mW/cm3(25℃)和80mW/cm3(100℃)；3MHz10mT条件下损耗为250mW/cm3(25℃)和150mW/cm3(100℃)，居里温度Tc＝270℃，电阻率ρ＝9Ω˙m，该材料μi较低，损耗较高。
专利(申请公开号CN105110785A)公开了“一种高频低损耗MnZn铁氧体及其制备方法”，其在100℃、1MHz30mT下功耗小于100mW/cm3，在25℃、3MHz10mT下功耗小于200mW/cm3，烧结温度为1180～1250℃，该材料室温下损耗较高，烧结温度也较高。专利(申请公布号CN102311263A)公开了“LED照明及开关电源变压器用高频低损耗高Bs铁氧体材料及其制备方法”，其μi＝1800±25％，Bs＝510mT(25℃)，100℃、500kHz50mT下功耗小于80mW/cm3；居里温度Tc＝260℃，电阻率ρ＝6.5Ω˙m，烧结温度为1300～1350℃，该材料损耗较高，烧结温度较高。专利(CN102503396A)公开了“一种高频低损耗MnZn铁氧体及其制备方法”，其μi＝1000，Bs＝450mT(25℃)，在100℃、1MHz30mT下功耗为100～160mW/cm3；其100℃、3MHz10mT下功耗为200～280mW/cm3，居里温度Tc＝260℃，烧结温度为1180～1250℃。
发明内容
本发明提供一种工作于0.5～3MHz的高频低损耗MnZn功率铁氧体材料及制备方法。
本发明解决所述技术问题采用的技术方案是，MnZn功率铁氧体材料由主料和掺杂剂组成，主料按照摩尔百分比计，以氧化物计算，包括：52～56mol％Fe2O3，5～11mol％ZnO，33～43mol％MnO。
掺杂剂按照重量百分比，以氧化物计算，包括：0.05～0.1wt％CaCO3，0.1～0.3wt％TiO2，0.1～0.3wt％Co2O3，0.01～0.1wt％SnO2，0.01～0.1wt％V2O5。
掺杂剂的重量百分比以主料的重量为基准，例如0.05～0.1wt％CaCO3，若主料重量为100g，则CaCO3加入量为0.05～0.1g。
本发明用符号“～”表示数值范围，范围皆包含端点值。例如52～56mol％Fe2O3，范围包含了52mol％和56mol％。
本发明提供一种工作于0.5～3MHz的高频低损耗MnZn功率铁氧体材料的制备方法，包括以下步骤：
(1)主料配方
采用52～56mol％Fe2O3，5～11mol％ZnO，33～43mol％MnO；
(2)一次球磨
将上述粉料放入球磨机内，加入等量去离子水，球磨1～4小时；
(3)预烧
将步骤(2)所得球磨料烘干，并在800～1000℃炉内预烧1～3小时；
(4)掺杂
将步骤(3)所得粉料按重量比加入添加剂：0.05～0.1wt％CaCO3，0.1～0.3wt％TiO2，0.1～0.3wt％Co2O3，0.01～0.1wt％SnO2，0.01～0.1wt％V2O5；
(5)二次球磨
将步骤(4)所得粉料放入球磨机中，按照一定料球比例混合，加入等量的去离子水，球磨2～5小时，最终粉体粒径为0.4～1μm；
(6)成型
将步骤(5)所得粉料按重量比加入8～16wt％有机粘合剂PVA，混合均匀，造粒后，在压机上将粉料用模具压制成Φ25mm×Φ15mm×8mm环形坯件；
(7)低温烧结
将步骤(6)所得样品至于气氛炉内烧结，在500℃～1000℃缓慢升温，升温段氧分压保持21％，在1100℃～1180℃保温段保温4～8小时，保温段氧分压1％～4％，在降温段进行平衡气氛烧结；
(8)测试
将步骤(7)所得样品进行电磁性能测试。测试样品电感L，样品的起始磁导率由下式计算得到：
Figure BDA0001603263620000031
其中L为样品的电感，N为绕线匝数，h为样品的厚度，D为样品的外径，d为样品的内径，f为测试的频率。测试条件为：f＝1kHz，U＝0.5V，绕线匝数为10匝。用岩崎SY-8232 B-H分析仪测试样品的功耗。测试条件为：500kHz50mT，1MHz30mT，3MHz10mT，测试温度为：25℃和100℃。饱和磁感应强度Bs、剩余磁感应强度Br和矫顽力Hc的测试条件为1kHz 1200A/m，测试温度为：25℃和100℃。
本发明研制的MnZn功率铁氧体材料，其烧结温度仅为1100℃～1180℃，具体性能指标参数如下：
起始磁导率μi：1400±20％；
饱和磁感应强度Bs：≥510mT(25℃)；≥420mT(100℃)；
损耗PL(500kHz50mT)：≤50kW/m3(25℃)；≤60kW/m3(100℃)；
损耗PL(1MHz30mT)：≤35kW/m3(25℃)；≤70kW/m3(100℃)；
损耗PL(3MHz10mT)：≤150kW/m3(25℃)；≤220kW/m3(100℃)；
居里温度Tc＞260℃；
电阻率ρ＞10Ω˙m；
密度dm：≥4.85g/cm3；
与上述材料相比，本发明有效降低了材料在MHz高频时的损耗，在0.5～3MHz的宽频范围和25～100℃的温度范围内都具有较低的功率损耗。同时，本发明提供的制备方法烧结温度低，具有节能和环保的优点。
本发明的要点在于，在适宜的主配方基础上，通过CaCO3、TiO2、Co2O3、SnO2、V2O5多种添加剂的复合掺杂，实现对材料微观形貌和磁性能的控制。具体来讲，掺入V2O5等低熔点添加剂形成液相烧结，有效促进烧结过程中固相反应的进行，降低烧结温度，实现低温烧结；掺入Ca2+富集于晶界，在晶界处形成高阻层，提高电阻率；掺入对Fe2+有束缚作用的Sn4+、Ti4+，使得Fe2+不能自由的参与导电，提高材料电阻率。最终，通过多种掺杂剂的复合加入，并按照一定的烧结工艺制备的MnZn功率铁氧体，密度高、气孔少、晶粒完整均匀，在0.5～3MHz的宽频范围和25～100℃的温度范围内都具有较低的损耗，能稳定应用于MHz级开关电源中。以下结合附图和具体实施方式对本发明作具体的说明。
附图说明
图1为工作于0.5～3MHz的高频低损耗MnZn功率铁氧体材料的断面SEM照片。
具体实施方式
高频低损耗MnZn功率铁氧体材料由主料和掺杂剂组成，主料按照摩尔百分比计，以氧化物计算，包括：
52～56mol％Fe2O3，5～11mol％ZnO，33～43mol％MnO。
掺杂剂按照重量百分比，以氧化物计算，包括：
0.05～0.1wt％CaCO3，0.1～0.3wt％TiO2，0.1～0.3wt％Co2O3，0.01～0.1wt％SnO2，0.01～0.1wt％V2O5。
高频低损耗MnZn功率铁氧体材料的制备方法，包括以下步骤：
(1)主料配方
采用52～56mol％Fe2O3，5～11mol％ZnO，33～43mol％MnO；
(2)一次球磨
将上述粉料放入球磨机内，加入等重量去离子水，球磨2小时
(3)预烧
将步骤(2)所得球磨料烘干，并在920℃炉内预烧2小时；
(4)掺杂
将步骤(3)所得粉料按重量比加入添加剂：0.05～0.1wt％CaCO3，0.1～0.3wt％TiO2，0.1～0.3wt％Co2O3，0.01～0.1wt％SnO2，0.01～0.1wt％V2O5。
(5)二次球磨
将步骤(4)所得粉料放入球磨机中，加入等重量的去离子水，在球磨机中球磨4h，最终粉体粒径约为0.95μm；
(6)成型
将步骤(5)所得粉料按重量比加入12wt％有机粘合剂PVA，混合均匀，造粒后，在压机上将粉料用模具压制成Φ25mm×Φ15mm×8mm环形坯件；
(7)低温烧结
将步骤(6)所得样品至于气氛炉内烧结，在500℃～1000℃缓慢升温，升温段氧分压保持21％，在1100℃～1180℃保温段保温4～8小时，保温段氧分压1％～4％。
对上述制备方法的组分进行优选形成实施例1～6，各步骤组份见下表：
Figure BDA0001603263620000051
(8)测试
将步骤(7)所得样品进行电磁性能测试。测试样品室温电感L，样品的起始磁导率由下式计算得到：
Figure BDA0001603263620000052
其中L为测试样品的电感，N为绕线匝数，h为测试样品的厚度，D为测试样品的外径，d为测试样品的内径，f为测试的频率。测试条件为：f＝1kHz，U＝0.5V，绕线匝数为10匝。用岩崎SY-8232 B-H分析仪测试样品的功耗和饱和磁感应强度。功耗的测试条件为：500kHz50mT，1MHz30mT，3MHz10mT，测试温度为25℃和100℃。饱和磁感应强度Bs、剩余磁感应强度Br和矫顽力Hc的测试条件为1kHz 1194A/m，测试温度为25℃和100℃。
实施例1-6的测试结果如下表：
Figure BDA0001603263620000053
Figure BDA0001603263620000061

Claims (2)

1.MHz级开关电源用MnZn功率铁氧体，其特征在于，由主料和掺杂剂组成，主料按照摩尔百分比计，以氧化物计算，包括：52~56mol%Fe2O3，5~11mol%ZnO，33~43mol%MnO；掺杂剂按照重量百分比，以氧化物计算，包括：0.05~0.1wt%CaCO3，0.1~0.3wt%TiO2，0.1~0.3wt%Co2O3，0.01~0.1wt%SnO2，0.01~0.1wt%V2O5，以上组分之和为100%。
2.MHz级开关电源用MnZn功率铁氧体的制备方法，其特征在于，包括以下步骤：
（1）主料配方
采用52~56mol%Fe2O3，5~11mol%ZnO，33~43mol%MnO；
（2）一次球磨
将上述粉料放入球磨机内，加入等重量去离子水，球磨1~4小时；
（3）预烧
将步骤（2）所得球磨料烘干，并在800～1000℃炉内预烧1~3小时；
（4）掺杂
将步骤（3）所得粉料按重量比加入添加剂：0.05~0.1wt%CaCO3，0.1~0.3wt%TiO2，0.1~0.3wt%Co2O3，0.01~0.1wt%SnO2，0.01~0.1wt%V2O5；
（5）二次球磨
将步骤（4）所得粉料放入球磨机中，按照一定料球比例混合，加入等量去离子水，在球磨机中球磨2~5小时，最终粉体粒径为0.4～1μm；
（6）成型
将步骤（5）所得粉料加入有机粘合剂，混合均匀，造粒，压制成坯件；
（7）低温烧结
将步骤（6）所得坯件在500℃~1000℃缓慢升温，升温段氧分压保持21%；在1100℃~1180℃保温段保温4～8小时，保温段氧分压1%～4%；在降温段进行平衡气氛烧结。
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